公开(公告)号：US20160096819A1

公开(公告)日：2016-04-07

申请号：US14890711

申请日：2014-05-16

Applicant: BASF SE

Inventor： Christopher KORADIN ,  Thomas ZIERKE ,  Ralf HOOCK ,  Karsten KOERBER

IPC: C07D401/04

CPC classification number: C07D401/04

Abstract: The present invention relates to a process for preparing N-substituted 1H-pyrazole-5-carboxylic acid compounds of the formula I-A and derivatives thereof, in particular the corresponding carbonylchloride compounds (acid chlorides). It also relates to the use of these acid chlorides for preparing anthranilamide derivatives that are useful pesticides. in which the variables are as defined in the claims and the specification comprising the steps of i) reacting a compound of the formula (II) with a base selected from combinations of a magnesium-organic compound having a carbon bound magnesium and a secondary amine and magnesium amides of secondary amines in the presence of a lithium halide, where the base is used in an amount sufficient to achieve at least 80% deprotonation of the compound of formula (II); and subjecting the product obtained in step (i) to a carboxylation by reacting it with carbon dioxide or a carbon dioxide equivalent, to obtain a magnesium salt of the compound of formula (I-A) and optionally aqueous workup to obtain the compound of the formula (I-A) as a free acid.

Abstract translation: 本发明涉及制备式I-A及其衍生物，特别是相应的碳酰氯化合物（酰氯）的N-取代的1H-吡唑-5-羧酸化合物的方法。 它还涉及这些酰氯用于制备有用农药的邻氨基苯甲酰胺衍生物的用途。 其中变量如权利要求和说明书中所定义，其包括以下步骤：i）使式（II）的化合物与选自具有碳结合的镁和仲胺的镁 - 有机化合物的组合的碱反应，以及 在卤化锂存在下，仲胺的胺化合物，其中碱的用量足以达到式（II）化合物的至少80％去质子化; 和通过使其与二氧化碳或二氧化碳当量反应使步骤（ⅰ）中获得的产物进行羧化，得到式（IA）化合物的镁盐，并任选地进行水处理，得到式 IA）作为游离酸。

公开(公告)号：US20160046644A1

公开(公告)日：2016-02-18

申请号：US14760302

申请日：2014-01-15

Applicant: BASF SE

Inventor： Melanie BONNEKESSEL ,  Wolfgang REICHERT ,  Ralf HOOCK ,  Thomas KAEDING ,  Christopher KORADIN ,  Andreas PLETSCH ,  Manfred EHRESMANN ,  Hartwig SCHROEDER

IPC: C07D493/04

CPC classification number: C07D493/04 ,  A01N43/90 ,  A01N53/00

Abstract: The present invention relates to a method for preparing the pyripyropene compound of the formula (I) which method comprises the following steps: i) subjecting a pyripyropene compound of formula Pyripyropene A to an alkaline hydrolysis to yield a 1,7,11-trideacetylpyripyropene A, ii) reacting 1,7,11-trideacetylpyripyropene A obtained in step i) with cyclopropane carbonyl chloride to yield a raw product containing the pyripyropene compound of formula (I); iii) subjecting the raw product of step ii) to crystallization to yield a crystalline pyripyropene compound of formula (I) and a mother liquor; and iv) recycling the mother liquor or a pyripyropene compound containing fraction thereof to the alkaline hydrolysis of step i).

Abstract translation: 本发明涉及一种制备式（I）的吡啶并苯化合物的方法，该方法包括以下步骤：i）使式Pyripyropene A的吡啶并吡喃化合物进行碱水解，得到1,7,11-三乙酰基吡啶 ，ii）使步骤i）中获得的1,1,11-三乙酰基吡啶并甲与环丙烷碳酰氯反应，得到含有式（I）的吡啶并吡喃化合物的粗产物; iii）使步骤ii）的粗产物进行结晶，得到式（I）的结晶吡啶并吡喃化合物和母液; 和iv）将含有其部分的母液或含吡啶并吡喃化合物再循环到步骤i）的碱水解。